Immiscible liquid countercurrent method and apparatus



April 1939- x M. D. MANN. JR 2,153,507

IMMISCIBLE LIQUID COUNTERGURRENT METHOD AND APPARATUS Filed Feb. 26, 1932 Patented 1939 i [2,153,507

UNITED STATES PATENT oFFicE IMMISCIBLE. LIQUID COUNTERGURRENT I METHODAND APPARATUS -Matthew D. Mann, Jr.,-Roselle, N. J., assignor to .Standard Oil Development Company, a corporation of Delaware Application February 26, 1932 Serial No. 595,330

'9 Claims. (Cl.v 23-270) This invention relates to counter-current tion to another through pip and is i treatment of fluids. The invention will be fully charged from the upp q Section t ou h a understood from the following description taken discharge line relatively heal/Y q in connection with the accompanying drawing, in Such as ap s t n containing pa afii is i 5 which latter 3 .troduced into the uppermost section through a 5 Fig. lis a longitudinal sectional view of .one line i at a rate of flow controlled by any suitable form of apparatus'suitable for carryi out the means, not shown. The relatively heavy liquid i nti v flows downwardly from one section to another Fig. 2 is a longitudinal sectional view of a through Pipes 3 and is discharged'from 1ihe 10 modified form f apparatus; and ermost section through a line 8. The-feed of rel- 10 i 3 is enlarged perspective View f am atively heavy and relativelyllght liquids into the other form of pipe shell can be a proportional rate of flow controlled 5 The invention is directed particularly to the as desiredcounter-current treatment of immiscible liquids In the operatlon of thls process the tower is of difierent gravities and will be described first filled with the relatively light liquid and the 15 illustration first in connection with the 'countertwo immiscible liquids are m Passed into the current treatment of soap solution, containing tOWer- The wnwardly flowing relatively heavy d ed pnraffin Wax, with naphtha s liquid is fed into the tower at a rate propormixtures are obtained in the manufacture of tional to the discharge through drains 6 and soaps from oxidized paramn wax, and require to cause accumulation of the heavy liquid above 20 purification by removal f Wax which has not each plate'in layers of substantial thickness. t i The depth of the heavy liquid layer above each Referring particularly to Fig 1 of the drawing, plate is controlled by the distance pipes 3 prothere is shown a tower, the shell of which is des- Ject above the plates The heavy nqmd gathignated by reference numeral. I. The shell is divided vertically into sections by means of a plulevel W the top of the plpes and neon flowmg rality of plates 2 which extend horizontally into plpe 3 is subdivided into drops by means of across the tower. One or more pipes 3, comthe Serrated jagged ends The size 9 h municating with openings in the plates 2, extend drops is governed by the dept}? of senjetlon m upwardly from each plate for a substantial dls- P ended the p plpes havmg holes 30 tame sumcient topermit the accumulation f a 1n the sides are used, the size of the holes govlayer of the heavy liquid, such as soap solution h drops pass dewnwerely through e c-ontaining parafflm The pipes 3 are provided I pipes 3 in contact with the relatiyely light liquid with openings for sub-dividing the heavy liquid passlPg upwardly, through sale pipes The into drops. In the embodiment illustrated in relatlvely heavy e passing downwardly from 35 Fig 1 the ends, of the pipes projectmg above the pipes 3 is diverted from direct flow to the the plates 2 are serrated or jagged to form the Pipes 3 of the Plate beneamby bamee e and openings to subdivide the heavy liquid into drops over the edges ofehe bemes flows to the cumulating area. In place of the baflles a similar as it enters the pipes from the accumulated layer. 40 Other means of subdividing the liquid may be effect may be Pmduced by arranging the PIPES 4o used suchas pipes having small openings or holes of 5 Plate that they are not directly in in the sides, through which openings the liquid lme Wlth the Plpes the Plates beneath and upon passing is divided into drops. Such a form above' is denotedby 3 m Fig 3 B ffles 4 in t f rm Numerous subdivisions of the relatively heavy of chimneys or plates may also be arranged beliquid flowing downwardly are thus made and 45 low each opening of thepipes 3, to deflect the better Contact With the light quid is accomdirect flow of the heavier from the pipes before the two are Withdrawn at in one'plate to the accumulating layer of the their e p c e drainsnext plate and also help the contact of the two Fig} 2 illustrates a od fied ounter-current immiscible liquids. scrubber where it is desirable to wash a lighter The relatively light liquid such as naphtha is liquid with water. For illustration, the lighter passed into the lowermost section through a line liquid s a ty acid containing Sulphuric acid 5 at a rate of flow controlled by any suitable and the heavier wash liquid is water. ,In this means, not shown. The relatively light liquid modified scrubber the shell is designated by flows upwardly through the shell from one secnumeral 9. The shell is divided vertically into 5 ered in a layer on the plates 2, upon rising to a 5 sections by means of a plurality of plates id which extend horizontally across the tower. One

or more pipes ll communicating with openings in the plates I I) extend downwardly from each plate for a substantial distance, sufficient to permit the accumulation of a layer of the lighter liquid passing upwardly through. the tower. .The ends I2 of the pipes projecting below the plates are serrated or jagged in form to subdivide the lighter liquid into drops as it passes into the pipes from the accumulatedlayer. Bailies It in the form of plates may also be arranged above each opening of the pipes II to deflect the flow of the lighter liquid from the pipes in one plate to the accumulating layer of the next plate above. In place of battles, an arrangement of the pipes'of each plate, so that they are not directly in line with the pipes of, the plates above and beneath, will produce the same effect.

There is provided an inlet ll for passing into the tower the heavier wash liquid and an outlet I5 for removing the heavier wash liquid with the impurities. Inlet I6 is used to pass the lighter liquid that is to be purified into the tower and outlet ll is used to remove the purified lighter liquid from the tower.

In the operation of this counter-current scrubber the tower is filled with the heavier liquid, water in-this case. The lighter liquid such as fatty acid containing sulphuric acid as an impurity is passed into the tower through pipe I6 and more water is also introduced through pipe I4. adjusted as desired and is governed by the purity of the fatty acids being removed through pipe 11. The fatty acid upon passing through the tower accumulates in layers beneath each plate and is subdivided into drops by means of the serrated end I2 of pipes II as it enters the pipes. The

drops flowing upwardly through the pipes H are brought into intimate contact with water flowing from opening H to drain IS. The purified fatty acid is withdrawn through drain l1 and the water with the sulphuric acid in solution is withdrawn through drain l5. 1

The examples given are for illustration only, as this apparatus may be used in any countercurrent purifying process, being limited only to two or more liquids which are immiscible with' each other and have enough difference inspecifl Other examples are:

Washing oil soluble sulphonlc acids from treated oilwith dilute alcohol. In this case the alcohol may have impurities which will be dissolved in the oil.

Acid treating of naphtha or oils.

In propane treating of lubricating oil stocks counter-current washing is necessary. Here temperature may be varied from top to bottom of the tower if desired. Ethane content of the solvent may be changed.

Emulsions are avoided in this process by regulating the number and the diameters oi the pipes used in intimately contacting the two liquids of different gravities.

The foregoing description is merely illustrative and various changes and alternative arrangements may be'm'ade within the scope of the appended claims in which it is my intention to claim all novelty inherent in the invention broadly as theprior art permits.

The rate of flow of the two liquidsmaybe grease? which comprises a substantially vertical shell, plates dividing the shell horizontally into sections, a pipe extending from an opening in each plate a substantial distance into an adjoining section, said pipe having serrations in its free end for sub-dividing the liquid into drops, both the uppermost and lowermost sections of the shell having an'inlet and an outlet.

2. Apparatus for the counter-current treatment of immiscible liquids of difierent gravities, which comprises a substantially vertical shell, plates dividing the shell horizontally into sections, a pipe extending from an opening in each plate a substantial distance into the adjoining section, the pipe being provided with a plurality of openings in its side wall for sub-dividing a liquid into drops, both the uppermost and lowermost sections of the shell having an inlet and'an outlet.

3. Apparatus for the counter-current treatment of immiscible liquids of difierent gravities, which comprises a substantially vertical shell, plates dividing the shell horizontally into sections, a pipe extending from an opening in each plate a substantial distance into an adjoining section, means provided on the pipes for subdividing a liquid into drops, baffles in each section to prevent direct flow of liquids between pipes in adjoining sections, both the uppermost and lowermost sections -of the shell having an inlet and an outlet.

4. In a process for treating a mineral oil with a solvent, the steps of continuously flowingsaid oil and solvent counter-currently through a contacting column, engaging the counter-currently flowing oil and solvent phases in a plurality of phase contacting paths of relatively small crosssectional area, and disengaging the oil and solvent phases to cause a layer formation thereof intermediate the ends of said column and between disconnected portions of said v paths.

5. In a process for contacting liquid phases such as in treating a mineral oil with a solvent, the steps of continuously flowing said phases counter-currentlythrough a contacting column, engaging the counter-currently flowing phases in a plurality of phase contacting paths of rela-' tively small cross sectional area, and disengaging the phases to cause at least one layer formation thereof intermediate the ends of said column and between disconnected portions of said paths.

6. In a process for treating a mineral oil with a solvent, the steps of continuously flowing said oil and solvent counter-currentlythrough a contacting column, engaging the counter-currently flowing oil and solvent phases in a'plurality of phase contacting paths of relatively small cross sectional area, and disengaging the oil and solvent phases to cause layer formations thereof at a plurality of spaced points intermediate the ends of said column and between disconnected portions of said paths.

7. In a. process for treating a mineral oil with a solvent, the steps of continuously flowing said oil and solvent counter-currently through a contacting column, engagingthe counter-currently flowing oil and solvent phases in a plurality of spaced sets of contacting paths of relatively small cross sectional area, feeding the solvent and oil phases into all paths of any one set at substantially the same ratio one to the other, and disengaging the oil and solvent phases between two adjacent sets of paths to cause a layer formation of said phases.

8. In combination, a column, means in said column for causing liquids to flow counter-currently through saldcolumn by virtue of a difler= ence in density such as in the treatment of mineral oils, means in said column for engaging the liquid phases in a plurality of sets of phase contacting paths of relatively small cross sectional area, and means for disengaging said phases intermediate said sets, and for causing at least one disengaged phase to assume a layer formation.

9. In a process for treating a mineral oil with a solvent, the steps of flowing said 011 and solvent counter-currently and serially through a plurality of spaced sets of phase contacting paths of relatively small cross sectional area, and causing layer formations at opposite ends of each set of phase contacting paths.

MATTHEW D. MANN, Jn. 

